CN109904431A - A kind of method of the modified cell positive material of mixed carbon source - Google Patents
A kind of method of the modified cell positive material of mixed carbon source Download PDFInfo
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- CN109904431A CN109904431A CN201910191863.4A CN201910191863A CN109904431A CN 109904431 A CN109904431 A CN 109904431A CN 201910191863 A CN201910191863 A CN 201910191863A CN 109904431 A CN109904431 A CN 109904431A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to anode material for lithium-ion batteries technical fields, disclose a kind of method of modified cell positive material of mixed carbon source.The method of the modified cell positive material of mixed carbon source of the present invention includes preparing LiFePO4 and/or phosphoric acid vanadium lithium presoma, thereafter mixed carbon source is added, successively pass through the ball milling of water and alcohol, and well-dried rear dry grinding obtains xerogel precursor mixture powder, thereafter, it is carried out to natural cooling after high-temperature calcination under inert gas or reducibility gas atmosphere, obtains the modified cell positive material of mixed carbon source.The method of the modified cell positive material of mixed carbon source of the present invention not only allows the uniformity of material to obtain the raising of high degree, but also every physical and chemical performance of the modified energy General Promotion positive electrode of mixed carbon source, overcomes the not high problem of finished product rate.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical fields, and in particular to a kind of modified anode of mixed carbon source
The method of material.
Background technique
Lithium ion battery passes through the development of many decades, has been widely used every field, including portable electronic device, mixed
Close power vehicle etc..However, the development of the negative electrode material in lithium ion battery either exists far ahead of positive electrode
On circulation ability, electric conductivity, quality or volume and capacity ratio, negative electrode material is better than anode, this is also at restriction lithium-ion electric
The key point of the application in pond.
Currently, modified cell positive material, which becomes, promotes cell positive material performance, the important of battery overall performance is promoted
Approach.Wherein, coated modified carbon is also most effective and simplest approach.However, excessive carbon adds during coated modified carbon
Enter, although the chemical property of positive electrode various aspects can be greatly promoted, also results in volume and capacity ratio reduction simultaneously, damage
The promotion of cell capacity.In addition, although phosphoric acid vanadium lithium and LiFePO4 are all very promising in lithium-ion-power cell
Positive electrode, but both materials of synthesis are produced in the market or their two-phase composite material all has finished product rate not
High problem.
Summary of the invention
The purpose of the invention is to overcome the shortcomings of above-mentioned background technique, a kind of modified anode of mixed carbon source is provided
The method of material.The present invention method modified by mixed carbon source not only allows material in conjunction with the technique of water for ball milling and alcohol ball milling
Uniformity obtain the raising of high degree, and overcome the modified bulk density that can reduce material of carbon or volume specific volume
The shortcomings that amount, General Promotion every physical and chemical performance of positive electrode, in addition, this method of modifying is low in cost, simple process
Controllably, there is great directive function to the production technology of existing industrialized production.
To achieve the object of the present invention, the modified cell positive material of mixed carbon source of the present invention method the following steps are included:
(1) LiFePO4 and/or phosphoric acid vanadium lithium presoma are prepared；
(2) xerogel precursor mixture is prepared: gained LiFePO4 and/or phosphoric acid vanadium lithium presoma in step (1)
Middle addition mixed carbon source heats up, and stirring obtains xerogel precursor mixture；
(3) dry after water for ball milling is added after being dried the middle gained xerogel precursor mixture of step (2), then plus
Enter alcohol ball milling, dry, dry grinding；
(4) it is transferred in heating furnace after dry grinding in step (3), 300 are warming up in inert gas or/and reducibility gas~
400 DEG C are sintered, heat preservation, natural cooling, obtained precursor powder；
(5) will be transferred in heating furnace after the grinding uniformly of precursor powder obtained in step (4), in inert gas or/and
700~850 DEG C are warming up in reducibility gas protective atmosphere, natural cooling after calcining at constant temperature obtains the modified electricity of mixed carbon source
Pond positive electrode.
In step (1) of the present invention phosphoric acid vanadium lithium presoma the preparation method comprises the following steps: by as the vanadium source compound of raw material,
P source compound, Li source compound, chelating agent are added in reaction vessel, and deionized water is added, and heat up, and stirring obtains vanadium phosphate
Lithium presoma.
Ferric lithium phosphate precursor the preparation method comprises the following steps: by the iron as LiFePO4 raw material in step (1) of the present invention
Source compound, P source compound, Li source compound, chelating agent are added in reaction vessel, add deionized water, heat up, stirring,
Obtain phosphoric acid vanadium lithium presoma.
Preferably, in the preparation method of LiFePO4 and/or phosphoric acid vanadium lithium presoma of the present invention, deionized water is added
After be warming up to 60~80 DEG C, 1~2h of magnetic agitation.
Preferably, lithium source chemical combination described in the preparation method of LiFePO4 and/or phosphoric acid vanadium lithium presoma of the present invention
Object is one of lithium dihydrogen phosphate, lithium carbonate, lithium nitrate, lithium hydroxide, lithium acetate or lithium sulfate or a variety of；The vanadium source
Closing object is one of vanadic anhydride or ammonium metavanadate or a variety of；Phosphorus source compound is lithium dihydrogen phosphate, biphosphate
One of ammonia, dihydrogen phosphate or ammonium phosphate are a variety of.
Preferably, ferro element, vanadium unit in the preparation method of LiFePO4 and/or phosphoric acid vanadium lithium presoma of the present invention
Element, P elements, elemental lithium and chelating agent molar ratio be (0.7~0.9): (0.1~0.3): (1~1.2): (1.1~1.3):
(2.5~3.5).
Preferably, chelating agent described in the preparation method of LiFePO4 and/or phosphoric acid vanadium lithium presoma of the present invention is
At least one of the hydrogen peroxide that oxalic acid, citric acid, tartaric acid, polyacrylic acid and mass ratio are 30%.
Mixed carbon source is inorganic carbon source and organic carbon source in step (2) of the present invention；Preferably, the inorganic carbon source is
At least one of acetylene black, graphene, graphite powder and superconduction carbon black, the organic carbon source are water-soluble sugar, such as sucrose, or
It is dissolved in the high-molecular compound of alcohol, such as polyethylene glycol.
It is further preferred that be formed by carbon coated shared in cell positive material for inorganic carbon source in the mixed carbon source
Mass percent be 1~5%, organic carbon source mass percent shared in cell positive material is 0.5~2%.
It is further preferred that the content of the carbon be the modified cell positive material quality of mixed carbon source of preparation 1.5~
7%.
It heats up, stirs after mixed carbon source is added in step (2) of the present invention, until the moisture in solution is evaporated.
60~80 DEG C are warming up to after mixed carbon source is added in step (2) of the present invention, 5~10h of magnetic agitation.
Preferably, it is dried and refers to gained xerogel presoma mixing in step (2) in step (3) of the present invention
After object is put into air dry oven or vacuum oven dry 10~20h.
Preferably, after water for ball milling refers to drying process in step (3) of the present invention, xerogel precursor mixture is put
Enter in the ball grinder of acid corrosion-resistant, such as in polyurethane or ceramic ball grinder, 2~4h of water for ball milling is added.
Preferably, the specific additional amount of water is after adding water for ball milling in water for ball milling in step (3) of the present invention, and presoma is mixed
Closing object and formed, there is 2~5 minutes water of mobility and standing will not be precipitated or be layered.
Preferably, in step (3) of the present invention alcohol ball milling be added 2~4h of alcohol ball milling, dry grinding the time be 0.3~
0.8h, such as 0.5h.
Preferably, the specific additional amount of alcohol is presoma mixing after alcohol ball milling is added in step (3) of the present invention
Object forms to have mobility and stand 2~5 minutes alcohol and will not be precipitated or be layered.
Preferably, in step (4) of the present invention in inert gas or/and reducibility gas atmosphere with 2~8 DEG C/min
Heating rate be warming up to 300~400 DEG C and be sintered, keep the temperature natural cooling after 3~5h.
Preferably, in step (5) of the present invention in inert gas or/and reducibility gas protective atmosphere with 2~8
DEG C/min heating rate is warming up to 700~850 DEG C, natural cooling after 8~12h of calcining at constant temperature.
Inert gas is argon gas in step (4) of the present invention and (5)；Reducibility gas is nitrogen, carbon monoxide or hydrogen
One of gas is a variety of, and when containing carbon monoxide or hydrogen in inert gas or/and reducibility gas, wherein nitrogen, hydrogen
Gas or carbon monoxide account for the 4~8% of mixed gas volume.
Preferably, heating furnace is tube furnace in step (4) of the present invention and (5).
Compared with the prior art, the advantages of the present invention are as follows:
1, the method that the present invention is modified cell positive material using mixed carbon source, and combine water for ball milling and alcohol ball milling, work
Skill is simple controllable, easily operated, and can apply to industrialization large-scale production, and the uniformity of material is not only allowed to obtain high degree
Raising, and mixed carbon source it is modified can General Promotion positive electrode every physical and chemical performance, overcome finished product rate not
High problem；
2, in the present invention, by the ball milling of water and alcohol, the dispersion performance of feed components and carbon is made to obtain very great Cheng
The raising of degree, to guarantee that the modifying function of carbon is protected；
3, the modified selected carbon source of the carbon in the present invention, raw material cost is low, from a wealth of sources, on the basis of modification,
The requirement for reducing cost is able to satisfy in industrialization large-scale production.
Detailed description of the invention
Fig. 1 is the XRD diagram for the mixed carbon source modified material that the embodiment of the present invention 1 obtains, and wherein abscissa is the 2 θ angles of diffraction,
Ordinate is relative intensity；
Fig. 2 is the TEM figure for the mixed carbon source modified material that the embodiment of the present invention 1 obtains, and wherein LVP is phosphoric acid vanadium lithium, KB
Carbon is section's qin superconduction carbon black；
Fig. 3 is the electrical property curve graph for the mixed carbon source modified material that the embodiment of the present invention 1 obtains；
Fig. 4 is the XRD diagram for the mixed carbon source modified material that the embodiment of the present invention 2 obtains, and wherein abscissa is the 2 θ angles of diffraction,
Ordinate is relative intensity；
Fig. 5 is the electrical property curve graph for the mixed carbon source modified material that the embodiment of the present invention 2 obtains, wherein horizontal in Fig. 5 (a)
Coordinate is specific discharge capacity, and ordinate is voltage, and in Fig. 5 (b), abscissa is circle number, and ordinate is specific discharge capacity.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.Additional aspect and advantage of the invention will be set forth in part in the description, part
It will become apparent from the description below, or practice through the invention is recognized.It is only used to solve it should be appreciated that being described below
The present invention is released, is not intended to limit the present invention.
Term "comprising" used herein, " comprising ", " containing " or its any other deformation, it is intended that covering non-exclusionism
Include.For example, composition, step, method, product or device comprising listed elements are not necessarily limited to those elements, but
It may include not expressly listed other elements or such composition, step, method, product or the intrinsic element of device.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
In addition, technical characteristic involved in each embodiment of the present invention as long as they do not conflict with each other can
To be combined with each other.
Embodiment 1
The preparation method of the mixed carbon source modified phosphate vanadium lithium/carbon composite material of the present embodiment the following steps are included:
(1) precursor preparation: by 2.5g V2O5, 5.1986g C2H2O4·2H2O, 4.2069g C2H7LiO4And 4.7430g
NH4H2PO4It is put into the beaker of the 500ml indigo plant lid bottle equipped with 300ml deionized water or 1L, two hours of 80 DEG C of heating stirrings
Afterwards, the yellow in solution completely disappears, and obtains blue-tinted transparent solution；
(2) section's qin superconduction carbon black of 1.1265g sucrose (organic carbon source) and 0.3111g will be added in the solution of above-mentioned (1)
(KB carbon, inorganic carbon source) continues heating stirring until becoming the xerogel precursor mixture of not mobility；
(3) it after being dried the precursor mixture of above-mentioned (2), moves into and 100mL deionization is added in high energy ball mill
After water for ball milling 2h, it is put into 80 DEG C of dryings in air dry oven and for 24 hours, 150mL alcohol ball milling 2h is added thereafter, is put into air dry oven
Middle drying about 6h, high-energy ball milling 0.5h, obtains phosphoric acid vanadium lithium/carbon precursor mixture powder again；
(4) by the precursor mixture powder in above-mentioned (3) in tube furnace, in the H of 95% Ar and 5%2Atmosphere is protected
Under shield, 350 DEG C, pre-burning 4h are warming up to the heating rate of 2~8 DEG C/min, natural cooling after 3~5h is kept the temperature, through high-energy ball milling 2
After hour, 800 DEG C are warming up to 2~8 DEG C/min heating rate in inert gas or/and reducibility gas protective atmosphere, perseverance
Temperature calcining 8h obtains the modified vanadium phosphate lithium/carbon composite material product of mixed carbon source after the completion again through high-energy ball milling 1 hour.
XRD result, TEM result and the electricity of vanadium phosphate lithium/carbon composite material made from preparation method using the present embodiment
Chemical property difference.By diffraction maximum position, intensity and width in Fig. 1 it can be concluded that synthesis produces
Product are the pure phases of phosphoric acid vanadium lithium, and crystallinity is also fine；It can see by the TEM in Fig. 2, phosphoric acid vanadium lithium surface is coated with one layer
The amorphous carbon layer of 1-2nm or so, and KB carbon is dispersed between particle, simultaneously synthesizing vanadium phosphate lithium/carbon composite material has non-
The chemical property of Chang Youyi (referring to Fig. 3).
Embodiment 2
A kind of modified lithium iron phosphate/lithium vanadium phosphate/carbon composite preparation method packet of mixed carbon source of the present embodiment
Include following steps:
(1) precursor preparation: by 0.2197g V2O5With 0.4569g C2H2O4·2H2O is put into beaker, and 800mL is added
Deionized water, 80 DEG C of heating stirrings are until solution becomes the VOC of blue-tinted transparent2O4After solution, 5.0543g is sequentially added
FeC2O4·2H2O、3.2501g CH3COOLi·2H2O and 3.6642g NH4H2PO4And 300mL deionized water, continue to heat
Stirring is up to solution surface layer is not it is observed that apparent bubble evolution；
(2) 0.2173g sucrose and 0.1200g section qin superconduction carbon black (KB are added in mixture obtained in Xiang Shangshu (1)
Carbon), continue heating stirring until the water in solution is evaporated completely the xerogel precursor mixture for becoming not mobility；
(3) it after being dried the mixture in above-mentioned (2), is put into the polyurethane ball-milling pot that capacity is 500L and is added
At the deionized water ball milling of 150mL 2 hours, 80 DEG C after forced air drying 24 hours, 200mL alcohol is added after the about 0.5h that dry grinds
Wet-milling 2h is carried out, ball grinder is put into baking oven, after 80 DEG C of sufficiently dry 10h, ball grinder is placed into high energy in ball mill
Ball milling 0.5h obtains precursor mixture powder；
(4) precursor mixture in above-mentioned (3) is put into tube furnace, in the H of 95% Ar and 5%2Atmosphere protection
Under, 350 DEG C are warming up to the heating rate of 2~8 DEG C/min, after pre-burning 4h, natural cooling after 3~5h are kept the temperature, through high-energy ball milling 2
After hour, 800 DEG C are warming up to 2~8 DEG C/min heating rate in inert gas or/and reducibility gas protective atmosphere, perseverance
Temperature calcining 10h, product cross 300 meshes after high-energy ball milling, and the bulky grain for failing sieving is repeated once high-energy ball milling and sieving step
Suddenly.Dusty material after sieving is the modified lithium iron phosphate/lithium vanadium phosphate/carbon composite wood of mixed carbon source made from this example
Material, wherein the mass ratio of LiFePO4 (LFP) and phosphoric acid vanadium lithium (LVP) is 9: 1, phosphorus content 1.5%.
Lithium iron phosphate/lithium vanadium phosphate/carbon composite XRD result made from preparation method using the present embodiment and
Chemical property difference is as shown in Figure 4 and Figure 5.By diffraction maximum position, intensity and width in Fig. 4 it can be concluded that sintetics
It is lithium iron phosphate/lithium vanadium phosphate/carbon composite material, and crystallinity is also fine；As shown in Figure 5, mixed carbon source of the present invention is modified
Lithium iron phosphate/lithium vanadium phosphate/carbon composite have very good chemical property.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of method of the modified cell positive material of mixed carbon source, which is characterized in that the described method comprises the following steps:
(1) LiFePO4 and/or phosphoric acid vanadium lithium presoma are prepared；
(2) it prepares xerogel precursor mixture: adding in gained LiFePO4 and/or phosphoric acid vanadium lithium presoma in step (1)
Enter mixed carbon source, heat up, stirring obtains xerogel precursor mixture；
(3) by after gained xerogel precursor mixture drying process in step (2), after water for ball milling is added, drying adds wine
Smart ball milling, dry, dry grinding；
(4) it is transferred in heating furnace after dry grinding in step (3), is warming up to 300~400 DEG C in inert gas or/and reducibility gas
It is sintered, keeps the temperature, natural cooling, obtained precursor powder；
(5) it will be transferred in heating furnace after the grinding uniformly of precursor powder obtained in step (4), in inert gas or/and reduction
Property gas atmosphere in be warming up to 700~850 DEG C, natural cooling after calcining at constant temperature is obtaining the modified battery of mixed carbon source just
Pole material.
2. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(1) in phosphoric acid vanadium lithium presoma the preparation method comprises the following steps: by as the vanadium source compound of raw material, P source compound, Li source compound,
Chelating agent is added in reaction vessel, adds deionized water, heats up, and stirring obtains phosphoric acid vanadium lithium presoma；The step (1)
Middle ferric lithium phosphate precursor the preparation method comprises the following steps: by the Fe source compound, P source compound, lithium source as LiFePO4 raw material
Conjunction object, chelating agent are added in reaction vessel, and deionized water is added, and heat up, and stirring obtains phosphoric acid vanadium lithium presoma；Preferably, institute
In the preparation method for stating LiFePO4 and/or phosphoric acid vanadium lithium presoma, 60~80 DEG C are warming up to after deionized water is added, magnetic force stirs
Mix 1~2h.
3. the method for the modified cell positive material of mixed carbon source according to claim 2, which is characterized in that the ferric phosphate
Li source compound described in the preparation method of lithium and/or phosphoric acid vanadium lithium presoma is lithium dihydrogen phosphate, lithium carbonate, lithium nitrate, hydrogen
One of lithia, lithium acetate or lithium sulfate are a variety of；The vanadium source compound is in vanadic anhydride or ammonium metavanadate
It is one or more；Phosphorus source compound be one of lithium dihydrogen phosphate, ammonium di-hydrogen phosphate, dihydrogen phosphate or ammonium phosphate or
It is a variety of；Preferably, ferro element in the preparation method of the LiFePO4 and/or phosphoric acid vanadium lithium presoma, vanadium, P elements,
The molar ratio of elemental lithium and chelating agent is (0.7~0.9): (0.1~0.3): (1~1.2): (1.1~1.3): (2.5~3.5)；
Chelating agent described in the preparation method of the LiFePO4 and/or phosphoric acid vanadium lithium presoma is oxalic acid, citric acid, tartaric acid, gathers
At least one of the hydrogen peroxide that acrylic acid and mass ratio are 30%.
4. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(2) mixed carbon source is inorganic carbon source and organic carbon source in；Preferably, the inorganic carbon source be acetylene black, graphene, graphite powder and
At least one of superconduction carbon black, the organic carbon source is water-soluble sugar, such as sucrose, or is dissolved in the macromolecule chemical combination of alcohol
Object, such as polyethylene glycol；It is further preferred that inorganic carbon source is formed by carbon coated in anode material in the mixed carbon source
Shared mass percent is 1~5% in material, organic carbon source mass percent shared in cell positive material is 0.5~
2%；It is further preferred that the content of the carbon is the 1.5~7% of the modified cell positive material quality of mixed carbon source of preparation.
5. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(2) it heats up, stirs after mixed carbon source is added in, until the moisture in solution is evaporated；Preferably, it is added in the step (2) mixed
60~80 DEG C are warming up to after closing carbon source, 5~10h of magnetic agitation.
6. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(3) drying process, which refers to, in is put into air dry oven or vacuum drying for gained xerogel precursor mixture in step (2)
Dry 10~20h in case；Preferably, after water for ball milling refers to drying process in the step (3), by xerogel precursor mixture
It is put into the ball grinder of acid corrosion-resistant, such as in polyurethane or ceramic ball grinder, 2~4h of water for ball milling is added；Preferably, the step
Suddenly in (3) in water for ball milling water specific additional amount be plus water for ball milling after, precursor mixture formed have mobility and stand 2~
Water will not be precipitated or be layered within 5 minutes.
7. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(3) alcohol ball milling is that 2~4h of alcohol ball milling is added in, and the dry grinding time is 0.3~0.8h, such as 0.5h；Preferably, the step
(3) the specific additional amount of alcohol is after alcohol ball milling is added in, and precursor mixture, which is formed, to be had mobility and stand 2~5 points
Clock alcohol will not be precipitated or be layered.
8. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(4) in inert gas or/and reducibility gas atmosphere with the heating rate of 2~8 DEG C/min be warming up to 300~400 DEG C into
Row sintering, keeps the temperature natural cooling after 3~5h.
9. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(5) 700~850 DEG C are warming up to 2~8 DEG C/min heating rate in inert gas or/and reducibility gas protective atmosphere in,
Natural cooling after 8~12h of calcining at constant temperature.
10. the method for the modified cell positive material of mixed carbon source according to claim 1, which is characterized in that the step
(4) and in (5) inert gas is argon gas；Reducibility gas is one of nitrogen, carbon monoxide or hydrogen or a variety of, and when lazy
Property gas or/and reducibility gas in contain carbon monoxide or hydrogen when, wherein nitrogen, hydrogen or carbon monoxide account for mixed gas
The 4~8% of volume；Preferably, heating furnace is tube furnace in the step (4) and (5).
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| CN111533108A (en) * | 2020-05-11 | 2020-08-14 | 蒋达金 | Method for preparing lithium cobalt phosphate by using waste lithium cobalt oxide |
| CN111883747A (en) * | 2020-06-24 | 2020-11-03 | 华南理工大学 | Method for preparing porous graphene coated lithium vanadium phosphate by recovering graphite cathode material from waste power battery |
| CN114094082A (en) * | 2021-11-22 | 2022-02-25 | 湖南裕能新能源电池材料股份有限公司 | Lithium vanadium phosphate-carbon composite cathode material, preparation method thereof, lithium ion battery and electric equipment |
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